10-14-04 03:01
No 535728
A buddy of SWIM's would like to report a dream he had the other night.. This was the first dream hes had and it was (by this bees standards) quite satisfying...
SWIM's buddy has been buzzing around the hive for around a year and finally decided to reduce something...he chose not to listen to the elderbees advice (large rxns 4 newbees) and proceeded with a 0.5g (HALF A GRAM! yeah, its stupid...) reduction as his first attempt... SWIM has a moderate amount of formal chemistry training (3rd year university chem student), which is likely responsible for his getting any product at all.. ANYHOW
It all began with the precursors...
MBRP - 0.5g
LGI2 - 0.6g
... and some (0.5g)pre-major-gak (ie eudragit shit) pseudo cleaned a-la-SPD with solvant washes, crystals were brilliant needles that sparkled in the light.
next the reaction, in a test tube, he combined the precursors and added roughly 5ml dH2O, covered with mini-balloon, and let simmer in an oil bath for just under 24 hours (~120C oil temp).
workup was preformed a-la-Geez with (solvant washes, a/b, water washes, titration...) and the final product was left to evaporate on a watchglass dish... Yield was around 200mg, 40% (by weight) or 44% (molar yeild) Product reportedly burned without leaving residue, and finally... BIOassay revealed wonderful results, with no hint of pseudo flavor (thisbees nightmare...)
SWIM's buddy informed him that subsequent reductions will be larger (NOT NANOS!), incorporating a condenser and steam distillation (in place of A/B) and a few ReXtals but SWIMs buddy figured that with such a small batch, mechanical loss would be too high
Thanks go out to Geez, ware, ChemoSabe, and a bunch of other bees that i cant think of right now...
Comments? Suggestions? Flames? Bring it on!
HAH!
(Hive Bee)
10-14-04 08:16
No 535771
and added roughly 5ml dH2O
Are you sure?? Do u mean .5mL?
incorporating a condenser and steam distillation (in place of A/B)
Good move. I would recommend steam distillation and an a/b on the freebase distillate. Then recrystalisation by dual solvent followed by crystal-growing by dissolving in sterile dH20 and leaving to evap undisturbed @ room temp until dry.
(Stranger)
10-14-04 09:05
No 535785
Yeah what biotechdude said, are you sure you put 5mls in? thats like a 20X excess of what should be put in.
If you just wrote it down wrong let us know but if you really put in 5 mls and your rxn was successful then its something we have to look at!
Im thinking that your rxn flask was quite large and alot of the water just condensed on the sides bringing the water ratio down to successful levels...
Anyway good work on the synth my man, now it wont be long before your cooking up 30gram batches ;) and tweaking those re-xs to get BEAUTIFUL crystals.
Good luck.
(Hive Bee)
10-14-04 11:35
No 535795
Supposed to be 0.5ml
thanks for the feedback guys!
HAH!
(Hive Addict)
10-14-04 23:51
No 535871
Looks like your friend did his homework proper. Like so many others don't.
I'm sure you'll now soon see the overall advantage to going "non-nano". In your case it was fine to do one as your first though.
Swims's buddy just yelled to me that your next assignment should bee the 10 gram batch. If you decide to take it.
This message will attempt self destruction in 10 seconds but will mosty likely fail in that attempt.
can't flush this